CN104241074A - Photo ionization mass spectrum device used for detecting products of laser heating reactor in situ - Google Patents
Photo ionization mass spectrum device used for detecting products of laser heating reactor in situ Download PDFInfo
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- CN104241074A CN104241074A CN201410488996.5A CN201410488996A CN104241074A CN 104241074 A CN104241074 A CN 104241074A CN 201410488996 A CN201410488996 A CN 201410488996A CN 104241074 A CN104241074 A CN 104241074A
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Abstract
The invention relates to a laser heating reactor and a photo ionization mass spectrum device used for detecting products in situ. The laser heating reactor is composed of a main cavity, a laser device, a thermodetector, a sample feeding mechanism and a mass spectrum instrument. The technologies such as laser heating, in-situ ultrasound molecular beam sampling and vacuum ultraviolet photo ionization mass spectrum diagnosis are combined, and a novel thermal chemical reaction experimental study technology suitable for the pressure scope from vacuum and barometric pressure to high pressure is provided. Lasers with adjustable power are used for evenly and rapidly heating a reaction substrate, the sample reaction time is shortened, and the secondary reaction is omitted; molecules can be cooled with the ultrasound molecular beam sampling technology, so that unstable intermediate bodies survive; the vacuum ultraviolet soft ionization technology is adopted in vacuum ultraviolet photo ionization mass spectra, fragments are prevented from being produced, and the reaction products can be detected in real time.
Description
Technical field
The invention belongs to thermal chemical reaction laboratory apparatus technical field, a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product be specifically related to.
Background technology
In thermochemical reaction process, reactant can produce a large amount of stable, unstable products, and real-time, online composition and the spatial distribution obtaining these products, has important meaning to the Detailed Chemical Kinetic Mechanism in research thermochemical process.
Thermal chemical reaction is carried out under the high temperature conditions, needs complete pyroreaction device and product sniffer.Resistance wire heats as heating element reactor by conventional high-temperature reactor usually, or directly utilizes the semi-conducting materials such as SiC as reactor, utilizes resistance heating to provide hot environment.But electric heating experimental provision exists some problems, as low in the efficiency of heating surface, temperature distributing disproportionation is even, easy pollution etc.
In addition, chemical kinetics research needs the information such as intermediate reaction product structure and concentration accurately, especially unstable free radical.In conventional pyroreaction device, the raw multiple impacts reaction of sample retention time long hair, outlet ends temperature gradient causes greatly the easy compound of free radical, cannot study the monomolecular reaction process in thermochemical reaction process.
At present, the analysis means of detection reaction product molecule structure, mainly comprises In situ spectroscopic diagnosis and sampling analysis method.In situ spectroscopic diagnosis is noiseless to reaction system, but can only measure minority species; Sampling analysis method general capillary or sampling cone sample product, and product is generally analyzed by mass spectrum (MS) or gas chromatograph-mass spectrometer (GC-MS) (GC-MS).Sampling analysis method is the unique method obtaining most intermediate information in thermochemical reaction process at present.But traditional GC-MS method uses electron impact ionization source (EI-MS) this " firmly " ionization mode to make determinand ionization, thus produces a large amount of fragment ion peaks, even cannot obtain the molecular ion peak of determinand, thus bring difficulty to qualitative.
Summary of the invention
In order to solve, the pressure limit that Conventional thermal experiment exists in research material thermochemical reaction process is narrow, the efficiency of heating surface is low, temperature distributing disproportionation is even, the residence time is long, secondary and the repeatedly deficiency such as more than reaction, the invention provides a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product.
A kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product comprises main cavity, laser, temperature measurer 31, sample introduction mechanism and mass spectrometer 62;
Described main cavity comprises ionization chamber 16, reative cell 14, vacuum linear driving mechanism 11, laser transmission pipe 12 and sampling cone 15;
Described ionization chamber 16 is adjacent with reative cell 14, and the two adjacent sidewall offers through thief hole, and described sampling cone 15 is located at the thief hole place of reative cell 14 side.
The top of described laser transmission pipe 12 is positioned at reative cell 14, and it is outside that bottom is positioned at reative cell 14, and bottom is arranged on vacuum linear driving mechanism 11; The upper end of laser transmission pipe 12 to be provided with at the bottom of reactive group 13,13 belows being positioned at sampling cone 15 at the bottom of reactive group; The bottom of the vacuum linear driving mechanism 11 corresponding with the lower end of laser transmission pipe 12 is provided with window 23; Laser transmission pipe 12 vertically moves under the effect of straight line driving mechanism, to change at the bottom of reactive group 13 with the distance of sampling cone 15; Correspondingly with window 23 establish speculum 22, the laser emitting mouth of described laser 21 and the reflecting surface of speculum 22 corresponding; Described reative cell 14 sidewall is provided with capacitive pressure transducer 41, reative cell aspiration pump group 42 and valve 43, reative cell 14 sidewall also offers thermometer hole, reative cell 14 outside corresponding with thermometer hole is provided with temperature measurer 31, temperature measurer 31 electrically connect laser o controller 32, and laser o controller 32 electrically connect laser 21;
Described sample introduction mechanism comprises sample channel 54 and flow controller 53, and the outlet of described sample channel 54 is positioned at the side of at the bottom of reactive group 13, and the inlet communication of sample channel 54 outlet of flow controller 53; Described flow controller 53 is positioned at the outside of reative cell 14, and the import of flow controller 53 is also communicated with respectively and supplies sample pipeline 51 and carrier gas channel 52; Sample to be analyzed and carrier gas are mixed through flow controller 53 and to be entered by sample channel 54 by the flow set at the bottom of the reactive group of reative cell 14 on 13;
The side of described ionization chamber 16 is provided with ionization pressure transducer 44 and ionization chamber aspiration pump group 45; The opposite side of ionization chamber 16 is located at by described mass spectrometer 62, and mass spectrometer 62 is connected with ionization chamber 16 by electro-ionic osmosis device 61, and electro-ionic osmosis device 61 one end is stretched in ionization chamber 16, and is positioned at the top of thief hole, and the other end stretches in mass spectrometer 62.Advantageous Effects of the present invention embodies in the following areas:
1. the present invention utilizes high power density laser to heat at the bottom of certain size reactive group, it can be made to rise to high temperature rapidly, and ensure that base reservoir temperature is evenly distributed.Moreover, laser beam is narrow, mobility strong, can greatly save reative cell spatial design, simplifies heating and temperaturel measurement mechanism.The most key, adopt laser heating technique, gaseous sample molecule is very short in the suprabasil residence time of heating, is monomolecular reaction process, thus significant to the unimolecular mechanism reaction in research thermochemical reaction process;
2. the present invention is by adopting the sampling cone of different opening diameter, has effectively isolated reaction chamber and detection chamber, and while making detection chamber maintain detection constant pressure, the pressure of reaction chamber greatly can adjust to atmospheric pressure even high pressure range in vacuum;
3. the present invention adopts molecular beam technique to sample thermal chemical reaction product, and utilizes that vacuum ultraviolet ionized mass spectrum (PIMS) carries out in real time product, on-line analysis.Vacuum ultraviolet ionized is a kind of " soft " ionization mode, it produces fragment ion hardly, is beneficial to and analyzes multicomponent system simultaneously, does not need chromatographic isolation, thus overcome the shortcoming that EI-MS fragment is many, GC separating rate is slow, achieve quick, original position on-line water flushing to multicomponent system.Vacuum ultraviolet ionized usual use vacuum UV lamp or vacuum ultraviolet (VUV) LASER and synchrotron radiation vacuum-ultraviolet light are as ionization source, and relatively, synchrotron radiation vacuum ultraviolet (VUV) brightness is high, energy resolution is high, tunable, are especially beneficial to the analysis of complex system.
Accompanying drawing explanation
Fig. 1 is experimental provision structural representation of the present invention.
Fig. 2 is LASER HEATING, ultrasound molecular beam sampler, photo ionization and electro-ionic osmosis process schematic.
Fig. 3 is the thermal decomposition product mass spectrogram of the benzene utilizing apparatus of the present invention to obtain.
Fig. 4 is benzene (Benzene) in the benzene thermal decomposition process utilizing apparatus of the present invention to obtain, diacetylene (Diacetylene) and acetylene (Acetylene) temperature variant molar fraction, and numerical simulation curve.
Sequence number in upper figure: vacuum-ultraviolet light 8, ion 9, vacuum linear driving mechanism 11, laser transmission pipe 12, at the bottom of reactive group 13, reative cell 14, sampling cone 15, ionization chamber 16, laser 21, speculum 22, window 23, high power laser 24, temperature measurer 31, laser o controller 32, capacitive pressure transducer 41, reative cell aspiration pump group 42, valve 43, ionization pressure transducer 44, ionization chamber aspiration pump group 45, for sample pipeline 51, carrier gas channel 52, flow controller 53, sample channel 54, electro-ionic osmosis device 61, mass spectrometer 62, conversion zone 71, ultrasonic molecular beam 72.
Embodiment
Below in conjunction with accompanying drawing, by embodiment, the present invention is further described.
Embodiment:
See Fig. 1, a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product, comprises main cavity, laser, temperature measurer 31, sample introduction mechanism and mass spectrometer 62.
Main cavity comprises ionization chamber 16, reative cell 14, vacuum linear driving mechanism 11, laser transmission pipe 12 and sampling cone 15; Described ionization chamber 16 is adjacent with reative cell 14, and the two adjacent sidewall offers through thief hole, and described sampling cone 15 is installed on the thief hole place of reative cell 14 side; Sampling cone 15 material is quartz, and top open pore size is 50 ~ 500 μm;
The top of described laser transmission pipe 12 is positioned at reative cell 14, and it is outside that bottom is positioned at reative cell 14, and bottom is arranged on vacuum linear driving mechanism 11; The upper end of laser transmission pipe 12 to be provided with at the bottom of reactive group 13,13 belows being positioned at sampling cone 15 at the bottom of reactive group; The bottom of the vacuum linear driving mechanism 11 corresponding with the lower end of laser transmission pipe 12 is provided with window 23; Laser transmission pipe 12 vertically moves under the effect of vacuum linear driving mechanism 11, to change at the bottom of reactive group 13 with the distance of sampling cone 15.
At the bottom of reactive group, 13 are made up of upper potsherd and lower potsherd, and the material of described lower potsherd is the material that absorptivity, thermal conduction rate are all higher, comprises carborundum, aluminium nitride, graphite etc.; The material of described upper potsherd is the ceramic material of reactionlessness, comprises Alpha-alumina, quartz etc.; Laser transmission pipe 12 lower end is arranged on vacuum linear driving mechanism 11; Correspondingly with window 23 establish speculum 22, the laser emitting mouth of described laser 21 and the reflecting surface of speculum 22 corresponding; Reative cell 14 sidewall also offers thermometer hole, and reative cell 14 outside corresponding with thermometer hole is provided with temperature measurer 31, and temperature measurer 31 electrically connect laser o controller 32, and laser o controller 32 electrically connect laser 21;
The temperature measuring 13 top reaction surfaces at the bottom of reactive group implemented by temperature measurer 31, and feed back to laser o controller 32, the latter is according to the relation of actual temperature and design temperature, change output frequency and the duty ratio of laser 21, regulation output power, by the bottom of reactive group 13 temperature stabilization at design temperature;
Described sample introduction mechanism comprises for sample pipeline 51, carrier gas channel 52, flow controller 53 and sample channel 54.The outlet of described sample channel 54 is positioned at the side of at the bottom of reactive group 13, and the inlet communication of sample channel 54 outlet of flow controller 53; Described flow controller 53 is positioned at the outside of reative cell 14, and the import of flow controller 53 is also communicated with respectively and supplies sample pipeline 51 and carrier gas channel 52; Sample to be analyzed and carrier gas are mixed through flow controller 53 and to be entered by sample channel 54 by the flow set at the bottom of the reactive group of reative cell 14 on 13.
Described reative cell 14 sidewall is provided with capacitive pressure transducer 41, reative cell aspiration pump group 42 and valve 43; The side of described ionization chamber 16 is provided with ionization pressure transducer 44 and ionization chamber aspiration pump group 45; Capacitive pressure transducer 41 measures reative cell 14 in real time, and pressure signal is fed back to valve 43 and according to the relation of real-time pressure and setting pressure, change its opening degree, change pump-line conductance and effective speed of exhaust, control reative cell 14 pressure stability in setting pressure; Reative cell aspiration pump group 42 is other vacuum pump groups such as rotary-vane vaccum pump group or dry pump; Ionization chamber aspiration pump group 44 is molecular pump unit; In experimentation, the pressure of described reative cell 14 is 200 Pa ~ 2 bar.
The opposite side of ionization chamber 16 is located at by described mass spectrometer 62, and mass spectrometer 62 is connected with ionization chamber 16 by electro-ionic osmosis device 61, and electro-ionic osmosis device 61 one end is stretched in ionization chamber 16, and is positioned at the top of thief hole, and the other end stretches in mass spectrometer 62; Described mass spectrometer 62 is time-of-flight mass spectrometer, ion trap mass spectrometer or quadrupole mass spectrometer etc.;
Fig. 2 schematically illustrates LASER HEATING, ultrasound molecular beam sampler, photo ionization and electro-ionic osmosis process.The high power laser 24 that laser 21 sends enters laser transmission pipe 12 by speculum 22 and window 23, to be radiated at the bottom of reactive group 13 and to make it be rapidly heated below; Meanwhile, sample to be transported at the bottom of the reactive group of heating on 13 by sample channel 54, in conversion zone 71, thermal chemical reaction occurs;
The vacuum linear driver 11 that at the bottom of reactive group, the height of 13 is connected by it regulates; The product of differing heights is sampled by sampling cone 15 and forms ultrasonic molecular beam 72, enters into ionization chamber 16; Ultrasonic molecular beam 72 is ionized by the vacuum-ultraviolet light 8 that vertical direction is introduced subsequently, and the ion 9 of generation is incorporated in mass spectrometer 62 by electro-ionic osmosis device 61 to be analyzed.
In this example, sample to be analyzed is benzene; At the bottom of reactive group, the temperature range of 13 is from room temperature to 1823 K, and the Stress control of reative cell 14 is at 6 kPa, and the pressure of ionization chamber 16 is 10
-2pa magnitude; At the bottom of reactive group, 13 is 1 mm with the distance of sampling cone 15; Vacuum-ultraviolet light 8 adopts synchrotron radiation vacuum-ultraviolet light, has installed the introducing devices such as monochromator between itself and this device, and vacuum ultraviolet (VUV) light energy is respectively 9.5 eV, 11.27 eV and 11.70 eV.
Fig. 3 gives benzene thermal decomposition product mass spectrogram under different vacuum ultraviolet (VUV) light energy when different temperatures.Wherein, Fig. 3 (a) is 13 temperature at the bottom of reactive group is under 1823 K conditions, synchrotron radiation photon energy is 9.5 eV, 11.27 eV and 11.70 eV time the mass spectrogram that obtains.In this example, along with vacuum ultraviolet (VUV) light energy increases, different benzene, diacetylene and the acetylene of ionization energy is ionized successively.Fig. 3 (b) is under 13 condition of different temperatures at the bottom of reactive group, the mass spectrogram that vacuum ultraviolet photon energy obtains when 11.70 eV, the figure illustrates the temperature variant trend of benzene thermal decomposition product.
Fig. 4 gives benzene (Benzene) in benzene thermal decomposition process, diacetylene (Diacetylene) and acetylene (Acetylene) temperature variant molar fraction and numerical simulation curve.In experiment and the decomposition path-ways demonstrating benzene (Benzene) → benzyne (Benzyne) → diacetylene (Diacetylene)+acetylene (Acetylene) in theory.Confirm the important function of apparatus of the present invention to the reaction of research thermal decomposition process unimolecular mechanism.
Claims (9)
1. for a Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product, it is characterized in that: comprise main cavity, laser, temperature measurer, sample introduction mechanism and mass spectrometer;
Described main cavity comprises ionization chamber (16), reative cell (14), vacuum linear driving mechanism (11), laser transmission pipe (12) and sampling cone (15);
Described ionization chamber (16) is adjacent with reative cell (14), and the two adjacent sidewall offers through thief hole, and described sampling cone (15) is located at the thief hole place of reative cell (14) side;
The top of described laser transmission pipe (12) is positioned at reative cell (14), and it is outside that bottom is positioned at reative cell (14), and bottom is arranged on vacuum linear driving mechanism (11); The upper end of laser transmission pipe (12) is provided with (13) at the bottom of reactive group, and at the bottom of reactive group, (13) are positioned at the below of sampling cone (15); The bottom of the vacuum linear driving mechanism (11) corresponding with the lower end of laser transmission pipe (12) is provided with window (23); Laser transmission pipe (12) vertically moves under the effect of straight line driving mechanism, changes the distance of (13) and sampling cone (15) at the bottom of reactive group; Correspondingly with window (23) establish speculum (22), the laser emitting mouth of described laser (21) and the reflecting surface of speculum (22) corresponding; Described reative cell (14) sidewall is provided with capacitive pressure transducer (41), reative cell aspiration pump group (42) and valve (43), reative cell (14) sidewall also offers thermometer hole, reative cell (14) outside corresponding with thermometer hole is provided with temperature measurer (31), temperature measurer (31) electrically connect laser o controller (32), and laser o controller (32) electrically connect laser (21);
Described sample introduction mechanism comprises sample channel (54) and flow controller (53), and the outlet of described sample channel (54) is positioned at the side of (13) at the bottom of reactive group, and the inlet communication of sample channel (54) the outlet of flow controller (53); Described flow controller (53) is positioned at the outside of reative cell (14), and the import of flow controller (53) is also communicated with respectively and supplies sample pipeline (51) and carrier gas channel (52); Sample to be analyzed and carrier gas mix through flow controller (53) and press the flow set and enter on (13) at the bottom of the reactive group of reative cell (14) by sample channel (54);
The side of described ionization chamber (16) is provided with ionization pressure transducer (44) and ionization chamber aspiration pump group (45); The opposite side of ionization chamber (16) is located at by described mass spectrometer (62), mass spectrometer (62) is connected with ionization chamber (16) by electro-ionic osmosis device (61), electro-ionic osmosis device (61) one end is stretched in ionization chamber (16), and is positioned at the top of thief hole, and the other end stretches in mass spectrometer (62).
2. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, it is characterized in that: (13) at the bottom of reactive group are made up of upper potsherd and lower potsherd, the material of described lower potsherd is the material that absorptivity, thermal conduction rate are all higher, includes but not limited to carborundum, aluminium nitride, graphite; The material of described upper potsherd is the ceramic material of reactionlessness, includes but not limited to Alpha-alumina, quartz.
3. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, is characterized in that: described flow controller (53) is gas flow controller or liquid flow controller.
4. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, it is characterized in that: the pressure of described reative cell (14) is 200 Pa ~ 2 bar, cover from vacuum to atmospheric pressure and high pressure range, described reative cell aspiration pump group (42) is other vacuum pump groups such as rotary-vane vaccum pump group or dry pump.
5. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, is characterized in that: the pressure of described ionization chamber (16) is 10
-2pa magnitude, described ionization chamber aspiration pump group (45) is molecular pump unit.
6. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, is characterized in that: the thief hole aperture at sampling cone (15) tip is 50 ~ 500 μm, and material is quartz.
7. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, it is characterized in that: described ionization chamber (16) is also provided with vacuum-ultraviolet light connector, introduce vacuum-ultraviolet light (8), the vacuum ultraviolet ionized product sampled through sampling cone (15); Vacuum-ultraviolet light (8) includes but not limited to discharge lamp, laser, synchrotron radiation light.
8. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, it is characterized in that: described electro-ionic osmosis device (61) comprises the battery lead plate of several pieces central through holes, ion is incorporated into mass spectrometer (62) from ionization chamber (16).
9. a kind of Photoionization Mass Spectrometry device for in-situ investigation LASER HEATING reactor product according to claim 1, is characterized in that: described mass spectrometer (62) is time-of-flight mass spectrometer, ion trap mass spectrometer or quadrupole mass spectrometer etc.
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| CN105717189A (en) * | 2016-02-17 | 2016-06-29 | 上海交通大学 | Device for in-situ detection of catalytic reaction intermediate and product and detection method |
| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
| CN107958833A (en) * | 2017-11-28 | 2018-04-24 | 厦门大学 | A kind of original position intermediate detection mass spectrometer |
| CN108074793A (en) * | 2016-11-17 | 2018-05-25 | 中国科学院大连化学物理研究所 | A kind of multi-mode mass spectrum ionization source of multicomponent sample analysis |
| CN109192648A (en) * | 2018-08-09 | 2019-01-11 | 金华职业技术学院 | A kind of free radical photoproduct test method |
| CN112924525A (en) * | 2021-01-29 | 2021-06-08 | 厦门大学 | In-situ mass spectrometry device and method for fullerene formation mechanism research |
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| CN105784917A (en) * | 2014-12-26 | 2016-07-20 | 中国科学院大连化学物理研究所 | Application of mass spectrometer to detection process of ionized intermediates in catalytic reaction |
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| CN108074793A (en) * | 2016-11-17 | 2018-05-25 | 中国科学院大连化学物理研究所 | A kind of multi-mode mass spectrum ionization source of multicomponent sample analysis |
| CN108074793B (en) * | 2016-11-17 | 2019-11-12 | 中国科学院大连化学物理研究所 | A kind of multi-mode mass spectrum ionization source of multicomponent sample analysis |
| CN107576717A (en) * | 2017-10-24 | 2018-01-12 | 中国科学技术大学 | A kind of in-situ detector for different diffusion length catalytic reaction gas phase intermediate products |
| CN107576717B (en) * | 2017-10-24 | 2019-10-25 | 中国科学技术大学 | A kind of in-situ detector being catalyzed reaction gas phase intermediate product for different diffusion lengths |
| CN107958833A (en) * | 2017-11-28 | 2018-04-24 | 厦门大学 | A kind of original position intermediate detection mass spectrometer |
| CN109192648A (en) * | 2018-08-09 | 2019-01-11 | 金华职业技术学院 | A kind of free radical photoproduct test method |
| CN109192648B (en) * | 2018-08-09 | 2023-09-15 | 金华职业技术学院 | Free radical photo-product testing method |
| CN112924525A (en) * | 2021-01-29 | 2021-06-08 | 厦门大学 | In-situ mass spectrometry device and method for fullerene formation mechanism research |
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